Farmaceutische Analyse, Faculteit Farmaceutische Wetenschappen, KU Leuven, Leuven, Belgium; National Organization for Drug Control and Research, Giza, Egypt.
J Sep Sci. 2013 Oct;36(20):3432-9. doi: 10.1002/jssc.201300630. Epub 2013 Sep 6.
A simple CE method was developed and validated for the simultaneous determination of chlordiazepoxide (CHL), amitriptyline, and nortriptyline (mixture I) or the determination of CHL and imipramine (mixture II) using the same BGE. Sertraline and amitriptyline were used as internal standards for the first and second mixtures, respectively. The method allows amitriptyline to be completely separated from its impurity and main metabolite nortriptyline, which can be quantified from 0.2 μg/mL. The separation was achieved using 20 mM potassium phosphate buffer pH 5 containing 12 mM β-cyclodextrin and 1 mM carboxymethyl-β-cyclodextrin. UV detection was performed at 200 nm and a voltage of 15 kV was applied on an uncoated fused-silica capillary at 25°C. These experimental conditions allowed separation of the compounds to be obtained in 7 min. Calibration graphs proved the linearity up to 40 μg/mL for CHL, up to 100 μg/mL for amitriptyline and imipramine, and up to 5 μg/mL for nortriptyline. The accuracy and precision of the method have been determined by analyzing synthetic mixtures and pharmaceutical formulations. The analytical results were quite good in all cases indicating that the method was linear, sensitive, precise, accurate, and selective for both mixtures.
建立并验证了一种简单的 CE 方法，用于同时测定氯氮卓（CHL）、阿米替林和去甲替林（混合物 I），或测定 CHL 和丙咪嗪（混合物 II），两种混合物均使用相同的 BGE。曲唑酮和阿米替林分别作为第一和第二混合物的内标。该方法可使阿米替林与其杂质和主要代谢物去甲替林完全分离，去甲替林可从 0.2 μg/mL 定量。使用含 12 mM β-环糊精和 1 mM 羧甲基-β-环糊精的 20 mM 磷酸钾缓冲液 pH 5 实现分离。在 25°C 下，于未涂层熔融石英毛细管上施加 15 kV 电压，在 200nm 处进行 UV 检测。这些实验条件可在 7 分钟内实现化合物的分离。校准曲线表明，CHL 的线性范围为 0 至 40 μg/mL，阿米替林和丙咪嗪的线性范围为 0 至 100 μg/mL，去甲替林的线性范围为 0 至 5 μg/mL。通过分析合成混合物和药物制剂确定了该方法的准确性和精密度。在所有情况下，分析结果都相当好，表明该方法对两种混合物均具有线性、灵敏、精确、准确和选择性。
